Noble Metals Recovery said:
When using iron to solve a problem, and after all the metals have dropped, can you now just use nitric to remove the base metals?
Yes, you can, and that's the recommended procedure, but you have to be wise about how you go about the process. In place of scrap steel, you can also use zinc, assuming you have it at your disposal. No need to get any if not. I'd also like to mention that this should not, in any way, be construed as a replacement for dissolving the values in AR, then precipitating them for final separation. It is a necessary step prior to that operation, to get rid of unwanted metals.
If, by chance, you intend to pursue this process, it might be wise for you to contact me on the side for a few pointers. It's dead easy, but you should do things in logical order in order to not further complicate the process.
Back to the material in question, if you have traces of chlorides present, it's possible to dissolve some of the values, so you don't get far ahead. If you have a lot of base metal, and you've fairly well dried the material prior to using nitric, you should be fine. To insure that you are, I had a tendency to incinerate everything between changes in acids if there was any chance of losing anything to early dissolution. That may or may not be an important step, depending on existing conditions.
I mention this for good reason. When you don't use primary processes, you included a lot of garbage in your AR solution that can be troublesome. I'm not implying that that is your fate, but lets assume, for purpose of discussion (and your education), that the material you've recovered, or are in process of refining, is contaminated in that fashion, and will yield a solution that will be difficult, if not impossible, to filter prior to precipitation. Here's what I used to do, a process that was never found in print, but provided a much needed addition to the procedure.
After the nitric digest, in which you'd have removed the majority of base metals, I would then incinerate the remains, after getting everything in a Sharkskin filter. They're tough and fairly open, so allow rapid filtration. I would then incinerate the entire lot, which, by now, is generally not much material. Once incinerated, I'd do a wash with HCL acid, which would dissolve the balance of substances that were troublesome, then follow up with a tap water wash. I would then dissolve the remains in AR, yielding a solution that was very clean, and easily filtered. The quality of gold from an operation such as this can be very good----especially if you use good gold washing techniques after precipitation.
You mention using a gold button to help get rid of the nitric acid. I guess the point is that the unused AR will attack the gold, thereby consuming the nitric acid?
That's correct. It was a procedure I employed routinely. In order to know what gold belonged where, I weighed the button prior to introducing it to the lot, then weighed it afterwards. That way you know how much gold you added to the process, in case the material in question is not yours, or you're trying to determine a yield of a given batch. It is important that you add additional HCL to this process, to insure that the nitric acid is consumed. You can tell by the reaction if it has been or not. If not, you'd see action at the button.
Do you do the standard 3 evaporations?
That's an interesting question. As much as I've read about refining, nowhere have I read that there must be 3 evaporations, and my experience dictates that's nonsense. One
proper evaporation is more than adequate. It should consist of introducing a few drops of H2SO4, which will expel any unwanted lead as lead sulfate, which will then be filtered from the gold solution upon final filtration, then evaporating until the solution changes color and is well condensed. Additional HCL would be added at this stage, which helps expel the nitric. If you work with relatively clean solutions, they turn from golden colored to deep red, then lean towards a blackened red color. Dirty solutions are affected by the contamination, but tend towards black, or even dark green. It's not quite as easy to know when you've finished with the evaporation process when you're working with dirty solutions, and they have a tendency to bake out on the evaporating dish if you go too far. You have to use care when evaporating towards dryness, for it happens quickly. Once evaporated, it stands to reason that you would add water (tap water is fine unless it's very heavily contaminated with metals) to the evaporated gold to your satisfaction. I kept mine fairly concentrated
to keep beaker size small. That isn't necessary, it just worked better for processing large amounts of gold in small vessels. I added ice to the solution prior to precipitation, which kept the solution from over heating. Precipitation is an exothermic reaction,
and will heat the solution to the point where it won't precipitate well when the concentration is high enough. Mine generally was, especially when re-refining.
As a side note, if you've read any of my posts, you're likely tired of hearing me constantly harp on Hoke's book. If you don't have it,
buy it! Not tomorrow, not next week, and not when you feel it might be convenient. Buy it NOW. You should look upon that book, or one its equal, as being just as important as having a tank of fuel in your automobile when you anticipate a trip. Without it, there are simply too many unknowns that will haunt you no end.
Almost everything I learned about gold refining came from that book, and it carried me through more than 20 years of refining. I recommend it highly---------and ----no------I am not connected with the book in any way aside from knowing it's the best text out there for a novice. It's written in plain English, with no nonsense instructions aside from her constant recommendation to use gasoline when incinerating. I hope you understand that's totally insane!
Hope this helps. I'm open to further questioning, assuming I've left you with more questions than answers.
Harold
Edit: corrected typo, and added new comments.